CN1818768A - 用于制造多色电泳显示器的方法 - Google Patents

用于制造多色电泳显示器的方法 Download PDF

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CN1818768A
CN1818768A CNA2004100327522A CN200410032752A CN1818768A CN 1818768 A CN1818768 A CN 1818768A CN A2004100327522 A CNA2004100327522 A CN A2004100327522A CN 200410032752 A CN200410032752 A CN 200410032752A CN 1818768 A CN1818768 A CN 1818768A
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cup
thermoplasticity
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染荣昌
陈美英
曾金仁
吴让二
臧宏玫
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HIBEX IMAGE LLC
E Ink California LLC
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Abstract

本发明涉及用于制造多色电泳显示器的方法,包括以下步骤:a)制备微型杯;b)将所述微型杯层叠一层正性光致抗蚀剂;c)将所述的正性光致抗蚀剂进行图形曝光,在预定区域中有选择地打开微型杯;d)将打开的微型杯用电泳流体填充,所述电泳流体包含分散于第一色的介电溶剂中的带电荷颜料微粒;e)将经填充的所述微型杯密封;f)在不同的区域中重复步骤c)至e),从而产生填充有不同颜色的电泳流体的微型杯组;以及g)如果有,则去除残留的正性光致抗蚀剂。该方法可通过辊对辊的方式连续地或半连续地进行用该方法制造的显示器可以达到仅一张纸的厚度,对于环境不敏感。该显示器的特点是薄、具柔韧性、耐用、易操作并且形式灵活。

Description

用于制造多色电泳显示器的方法
发明背景
a)本发明所属的技术领域
本发明涉及一种电泳显示器,它包含对形状、尺寸、和纵横比有明确定义的盒,该盒用分散在溶剂中的带电荷颜料微粒填充;本发明还涉及制造这种显示器的新颖方法。
b)与本发明相关的背景技术
该电泳显示器是根据悬浮在溶剂中的带电荷颜料微粒的电泳现象制成的一种非发射性的装置。这种电泳显示器在1969年被首次提出。该显示器通常包含具有电极的两块板,这两块板彼此相对放置并由间隔物分隔开。该电极板中的一块通常是透明的。一种包含有一经过染色的溶剂和带电荷颜料微粒的悬浮物被封装在该二电极板之间。当在二个电极之间施加一个电压差时,该颜料微粒将迁移到一侧,该颜料的颜色或该溶剂的颜色依电压差的极性显现。
为了避免不希望的微粒移动(诸如沉淀),有人提出将二个电极之间的空间分成较小的单元。然而,在分隔式电泳显示器的情况下,在制作分隔物和悬浮物密封的过程中会遇到一些问题。另外,在分隔式电泳显示器中,不同颜色的悬浮物也很难彼此分离。
后来,有人尝试把悬浮物密封在微胶囊中。美国专利第5,961,804号以及第5,930,026号对微胶囊化的电泳显示器进行了说明。所述作为参考的显示器具有基本二维的微胶囊排列,每个微胶囊具有包含一种介电流体和一种带电荷颜料微粒悬浮物(在视觉上与介电溶剂对比)的电泳液组成。该微胶囊可以通过界面聚合、原位聚合,或其它已有的方法(例如物理制程、液体内固化或简单/复杂凝聚)来形成。在其形成后,该微胶囊可被注入到装有二个被间隔开的电极的盒中,或被“印刷”或被涂布到一透明导电膜上。该微胶囊也可被固定在一透明基材或夹在二电极之间的粘合剂中。
利用这些现有工艺方法,特别是美国专利第5,930,026号、第5,961,804号以及第6,017,584号所披露的微胶囊方法制备的电泳显示器有许多缺点。例如,用微胶囊方法制造的电泳显示器,由于微胶囊壁的化学性质受到对环境变化的敏感度(特别是对于湿度与温度的敏感度)的不利影响。第二,基于该微胶囊制作的电泳显示器,由于微胶囊的薄壁和大颗粒尺寸而具有不佳的抗刮性。为改进该显示器的操作性,微胶囊被嵌埋于大量的聚合物基材中。但是,由于二电极间距增大,使反应时间变长。因为电荷控制剂在该微胶囊制造期间倾向于扩散到水/油界面,所以也很难增加该颜料微粒上的表面电荷密度。在该微胶囊中颜料微粒的低电荷密度或ζ电位也会使响应速率降低。此外,因为微胶囊的大微粒尺寸和与大范围分布,对于色彩应用而言,此类型的现有技术的电泳显示器具有的分辨率与寻址能力较低。
本发明简述
本发明的第一个方面是关于一种电泳显示器,它包括形状、尺寸、和纵横比有明确定义的盒。该盒用分散在介电溶剂中的带电荷颜料微粒填充。
本发明另一个方面,提供了一种用于制造该电泳显示器的新颖的制造工艺。
本发明另一个方面,提供了具有明确定义的形状、尺寸、和纵横比的盒的制备方法。该盒将分散在介电溶剂中的带电荷颜料微粒密封,并由根据本发明所制作的微型杯构成。简言之,制备微型杯的方法包括用一个预成形的凸模,将涂布在一导电膜上的一热塑性或热固性前体物层进行模压;接着用辐射、冷却、溶剂蒸发、或其它方法使该热固性前体物层硬化;在硬化期间或之后,将其脱模。此外,该微型杯的形成可以通过将涂有辐射固化层的导电膜进行图形曝光,然后在该曝光区域变硬后,去除未曝光区域。
耐溶解且热机械稳定的微型杯所具有的尺寸、形状、和开口比例范围很宽,可以用上述两种方法中任一种方法制作。然后用在介电溶剂中的带电荷颜料微粒悬浮物填充该微型杯并密封。
本发明的另一个方面,是对填充有悬浮在介电溶剂中的带电荷颜料微粒分散物的电泳流体的微型杯提供密封方法。可以通过多种方法完成密封。优选的是,在该填充步骤之前,将一种热塑性或热固性前体物分散在该电泳流体中。该热塑性或热固性前体物与该介电溶剂不互溶,并具有比该溶剂和颜料微粒低的比重。在填充后,热塑性或热固性前体物将与电泳流体相分离,并在该流体的表面形成一漂浮层。然后,通过溶剂蒸发、界面反应、湿气、热或辐射,使该前体物层硬化,很容易地完成微型杯的密封。虽然可以使用二个或多个上述固化机理的组合来增加密封生产能力,但是优选为紫外光(UV)辐射方法。此外,该密封可以通过将包含有该热塑性或热固性前体物的溶液涂布在该电泳流体上完成。然后通过溶剂蒸发、界面反应、湿气、热、辐射或固化机理的组合方法,使该前体物层硬化而完成密封。这些密封方法是本发明的独特特征。
本发明的另一个方面,提供一种用于制造包含有明确定义的形状和尺寸的盒的单色电泳显示器的多步骤方法。该处理步骤包括使用上述的任何方法之一制备微型杯,将微型杯密封,以及最后用预涂布胶层的一第二导电膜与已经密封的微型杯阵列层叠。这种多步骤处理可以通过辊对辊的方式连续进行。
本发明的另一个方面提供一种用于制造全彩电泳显示器的方法,通过使用一正性作用的光致抗蚀剂层叠在预成形的微型杯上;通过将正性光致抗蚀剂图形曝光,然后显影光致抗蚀剂,选择性地打开一定数量的微型杯;使用着色的电泳流体填充已经开启的微型杯;用一种密封方法将已填充的微型杯密封。这些步骤可以重复,以形成填充不同颜色电泳流体的密封微型杯。
所披露的这些多步骤方法,可以通过辊对辊的方式连续地或半连续地进行。因此,这些方法适用于大批量低成本的生产。而且与其它大量生产操作工艺相比,这些方法的效率高并且成本低。根据本发明所制作的电泳显示器对于环境,特别是对于湿度和温度不敏感。该显示器的特点是薄、具柔韧性、耐用、易操作并且形式灵活。因为根据本发明所制作的电泳显示器包含纵横比令人满意且对形状和尺寸有明确定义的盒,所以该双重稳定反射式显示器具有极佳的色彩寻址能力、高对比度、以及快的切换速率。因此,消除了在先技术的电泳显示器的缺点。
附图简要说明
图1是本发明的电泳显示器的示意图。
图2a与2b图示用于电泳显示器制造的辊对辊工艺,特别是通过将涂布有一紫外光可固化组分的导电膜进行模压制作微型杯。
图3a至3d说明一种制作微模压用凸模的典型方法。
图4a至4c表示一种通过微模压所制作的典型的微型杯阵列。
图5a至5c表示通过对涂布有一层紫外光辐射热固性前体物的导电膜进行图形曝光制作微型杯的其它制作步骤。
图6是制作黑/白电泳显示器或其它单色电泳显示器的流程图。
图7a至7h是用于制作多色电泳显示器的流程图。
本发明详述
定义
除非在本专利说明书中另有定义,否则在此所有的技术术语都是根据本领域一般技术人员所通常使用和理解的惯用定义来使用。
术语“微型杯”是指通过微模压或图形曝光所制作的杯状凹处。
在本专利说明书中,术语“盒”所要表达的是指由一个密封的微型杯所形成的一个单位。该盒以分散在溶剂或溶剂混合物中的带电荷颜料微粒填充。
术语“明确定义”在说明该微型杯或盒时,意指该微型杯或盒具有根据本方法的特定参数所预先确定的明确形状、尺寸、和纵横比。
术语“纵横比”是电泳显示器技术中所通常熟知的术语。在本专利说明书中,它是指该微型杯的深度与宽度或深度与长度的比例。
优选实施例
如图1所示,本发明的电泳显示器包含有二个电极板(10,11)(至少其中之一是透明的(10)),和一层装在该二个电极之间的盒层(12)。该盒具有明确定义的形状和尺寸,并用分散在经着色的介电溶剂中的带电荷颜料微粒填充。当在两个电极之间施加一个电压差时,该带电荷微粒迁移到一侧,可以通过透明导电膜看见颜料或溶剂的颜色。至少两个导体之一是预制图形的。用于制备此类电泳显示器的方法包括很多方面。
I微型杯的制备
I(a)用模压法制备微型杯
加工步骤见图2a和图2b。凸模(20)可以放置在腹板(24)上方(图2a)或下方(图2b)。该透明导电极板是通过在一玻璃板或塑料板上涂布一层透明导电膜(21)制成。然后把一热塑性或热固性前体物层(22)涂布在该导电膜上。该热塑性或热固性前体物层在高于其玻璃化温度下,用辊、板、或带型凸模进行模压。用于制作该微型杯的热塑性或热固性前体物可以是多官能团的丙烯酸酯或甲基丙烯酸酯、乙烯醚、环氧化物以及它们的低聚物、聚合物和与类似物。优选的是多官能团丙烯酸酯及其低聚物。为获得理想的物理机械性能,多官能团环氧化物和多官能团丙烯酸酯的组合也非常有用。通常也加入诸如氨基甲酸乙酯丙烯酸酯、或聚酯丙烯酸酯等增强挠性的可交联低聚物,以增强模压制成的微型杯的弯曲强度。该组分可包含聚合物、低聚物、单体与添加剂,或者仅有低聚物、单体与添加剂。这种材料的玻璃化温度(Tg)通常在约-70℃150℃的范围,优选为约-20℃至50℃。该微模压制作通常在高于玻璃化温度的温度下进行。一个经过加热的凸模或一个经过加热的底板(模具靠在其上进行模压)可以用来控制微模压的温度和压力。
如图2a与图2b所示,在该热固性前体物层硬化的期间或之后,将该凸模脱模,显现出微型杯阵列(23)。该前体物层的硬化可通过冷却、辐射、热或湿气引发交联来完成。如果该热固性前体物的固化是通过紫外光辐射来完成,则紫外光可以从腹板的底部或顶端照射在透明导电膜上,如二图中所示。此外,紫外光灯可以安装在该模具内部。在这种情况中,模具必须是透明的,以使紫外光可以透过预成型的凸模辐射热固性前体物层。
凸模的制备
凸模可以通过光致抗蚀剂处理,然后进行蚀刻或电镀来制备。图3给出一种用于制备凸模的代表性实施例。使用电镀(图3a),在一玻璃基板(30)上喷镀一层籽金属薄层(31)(通常为3000),例如铬镍铁合金(chrome inconel)。接着涂布一层光致抗蚀剂层(32),并用紫外光曝光。在该紫外光与光致抗蚀剂层(32)之间放置一个光掩模(34)。该光致抗蚀剂的曝光区域变硬。然后用适当的溶剂清洗,去除未曝光区域。烘干剩下的硬化光致抗蚀剂,并再次喷镀一层籽金属薄层。然后一主模(图3b)就制备好了,可以进行电铸。用于电铸成形的典型材料是镍钴合金(33)。此外,该主模可由镍制作,如摄影光学仪器工程师学会会刊卷1663,pp.324(1992)中《薄镀层光学介质的连续制作》(“Continuousmanufacturing of thin cover sheet optical media”,SPIE Proc.)中所说明的,采用氨基磺酸镍(nickel sulfamate)电铸或无电镍沉积。该模具(22)的底板通常约50至400微米。该主模也可用其他微工程技术制作,包括电子束写入、干式蚀刻、化学蚀刻、激光写入或激光干涉,如《精密光学复制技术》见摄影光学仪器工程师学会会刊(“Replication techniques for micro-optics”,SPIE Proc.)卷3099,pp.76-82(1997)中说明。此外,该模具可使用塑料、陶瓷、金属,利用光加工制作。
图4a是通过微模压所制作的典型微型杯的光学轮廓测量的三维轮廓。图4b是表示该微型杯开口的光学显微照片俯视图。图4c是表示其深度的一列微型杯的光学轮廓纵向剖面视图。
I(b)通过图形曝光制作微型杯
作为另一种制作微型杯的方法,可以利用紫外光或其它形式的辐射,穿过光掩模(50),将涂布在导电膜(52)上的辐射固化材料(51)进行图形曝光(图5a)。该导电膜(52)涂布在塑料基板(53)上。
就辊对辊的工艺来说,光掩模可与腹板同步,即以与腹板相同的速度移动。在图5a的光掩模(50)中,深色的方块(54)代表不透明的区域,而该深色方块之间的空间(55)则代表无遮挡的区域。紫外光穿过无遮挡的区域(55)照射在辐射固化材料上。经曝光的区域变硬,然后将未曝光区域(光掩模的不透明区域所保护的)用适当的溶剂或显影剂去除,形成微型杯(56)。该溶剂或显影剂选自丁酮、甲苯、丙酮、异丙醇或类似物等通常用于溶解或降低辐射固化材料粘性的物质。
图5b和图5c说明用图形曝光制备微型杯的其它两种可选方法。此二图示的特点基本与图5a相同,对应的组件也用相同的数字标示。在图5b中,所使用的导电膜(52)不透明并且已预制图形。在这种情况下,利用导体图案作为光掩膜对感光材料进行图形曝光是有利的。在紫外光辐射后,去除未曝光区域,制成微型杯(56)。在图5c中,导电膜(52)也是不透明且有区带画案。通过作为第一光掩模的区带图案导电膜(52)从底部使该辐射固化材料曝光。从另一侧通过具有与该导电膜的区带垂直的区带图案的第二光掩模(50),进行第二曝光。然后用溶剂或显影剂去除未曝光区域,显露出微型杯(56)。
通常,该微型杯可以是任意形状的,且其尺寸与形状可以改变。在一个系统中,该微型杯可以具有大致相同的尺寸和形状。然而,为了使光学效果最大化,可制作形状和尺寸不同的混合微型杯。例如,用红色分散物填充的微型杯可以与绿色微型杯或蓝色微型杯具有不同的形状或尺寸。此外,一个像素可由不同个数的不同颜色的微型杯组成。例如,一个像素可由多个小的绿色微型杯、多个大的红色微型杯、以及多个小的蓝色微型杯组成。三种颜色不必具有相同的形状和数目。
该微型杯的开口可以是圆形、正方形、长方形、六角形或任何其它形状。开口之间的间隔区域最好小一些,以便在维持理想的机械性质的同时,获得较高的色彩饱和度和对比度。因此,蜂巢状开口比其它形状(例如圆形)开口更好。
对于反射式电泳显示器而言,各个微型杯的尺寸可在约102至约5×105平方微米的范围内,优选为约103至约5×104平方微米。微型杯的深度在约3至约100微米的范围内,优选为约10至约50微米。开口对壁的比例在约0.05至约100的范围内,优选为约0.4至约20。开口的距离(由开口的边缘至边缘的距离)通常在约15至约450微米的范围内,优选约25至约300微米。
II悬浮物/分散物的制备
用分散在介电溶剂中的带电荷颜料微粒填充微型杯。该分散物可根据现有的方法制备,例如披露于美国专利第6,017,584号、第5,914,806号、第5,573,711号、第5,403,518号、第5,380,362号、第4,680,103号、第4,285,801号、第4,093,534号、第4,071,430号、第3,668,106号,电气和电子工程师协会会刊《电子装置》(IEEETrans.Electron Device),ED-24,827(1977),以及J.Appl.Phys.49(9),4820(1978)。该带电荷的颜料微粒与其所悬浮的介质在视觉上形成反差。该介质是介电溶剂,最好具有低粘度且介电常数在约2至约30,对于高的微粒移动率而言,优选为约2至约15。适当的介电溶剂的实施例包括有十氢化萘(DECALIN)、5-亚乙基-2-降冰片烯、脂肪油、蜡下油等碳氢化合物;甲苯、二甲苯、苯基二甲苯乙烷、十二烷基苯和烷基萘等芳香族碳氢化合物;全氟萘烷、全氟甲苯、全氟二甲苯、二氯化三氟甲苯(dichlorobenzotrifluoride)、3,4,5三氯化-三氟甲苯(3,4,5-trichlorobenzotrifluoride)、氯五氟基苯(chloropentafluoro-benzene)、二氯壬烷、五氯苯等卤化溶剂;自明尼苏达州圣保罗(St.Paul)的3M公司的全氟溶剂,例如FC-43、FC-70和FC-5060;来自俄勒岗州波特兰(Portland)的TCI America公司的低分子量的含卤素的聚合物,例如聚全氟丙烯基醚(poly(perfluoropropylene oxide);来自新泽西州River Edge的Halocarbon Product公司的聚氯三氟乙烯poly(chlorotrifluoroethylene),例如卤烃油(Halocarbon oil);全氟化聚烷基醚(perfluoropolyalkylether),例如来自Ausimont公司的Galden或是来自特拉华州DuPont的Krytox Oils和油脂K-流体系列。在一个优选实施例中,使用聚氯三氟乙烯作为介电溶剂。在另一优选实施例中,使用聚全氟丙烯基醚做为介电溶剂。
该悬浮介质可为染料或颜料所着色。非离子偶氮与蒽醌染料特别地有用。有用的染料的例子非限定性地包括:亚利桑那州PylamProducts公司生产的油溶红EGN(Oil Red EGN),苏丹红(SudanRed),苏丹蓝(Sudan Blue),油溶蓝(Oil Blue),Macrolex Blue,溶剂蓝35(Solvent Blue 35),亚利桑那州Pylam Products公司的PylamSpirit黑和Fast Spirit黑,Aldrich公司的苏丹黑B(Sudan Black B),BASF公司的Thermoplastic Black X-70,以及Aldrich公司的蒽醌蓝,蒽醌黄114,蒽醌红111,135,蒽醌绿28。对于不溶性颜料的情形,用于使介质产生颜色的颜料颗粒亦可分散于该介电介质中。这些有色颗粒优选为不带电荷的。如果用于在介质中产生颜色的颜料颗粒是带电荷的,则其最好带有与该带电荷颜料微粒相反的电荷。若二种颜料微粒带有相同的电荷,则其应具有不同的电荷密度或不同的电泳移动速率。在任何情况下,用于产生介质颜色的染料或颜料必需具有化学稳定性,并与悬浮物中的其它组分相容。
该带电荷颜料微粒可为有机或无机颜料,如自Sun化学制品公司的TiO2、酞菁蓝(phthalocyanine blue)、酞菁绿(phthalocyaninegreen)、二芳基黄(diarylide yellow)、二芳基AAOT黄(diarylideAAOT Yellow)、喹吖啶酮(quinacridone)、偶氮(azo)、若丹明(rhodamine)、苝系颜料(perylene pigment series);自Kanto化学制品公司的汉撒黄G(Hansa yellow G)颗粒,以及Fisher公司的碳灯黑(Carbon Lampblack)。优选的是亚微粒子尺寸。该微粒应具有可接受的光学特性,不应被介电溶剂膨胀或软化,并且应该是化学稳定的。在正常的工作条件下,所产生的悬浮物亦必须稳定且能抗沉淀、乳化或凝结。
该颜料微粒可以本身带有电荷,或可以使用电荷控制剂使之明显带电,或悬浮在介电溶剂中时获得电荷。适当的电荷控制剂是本技术领域所熟知的;它们可以是聚合或非聚合性质,也可以是离子化或非离子化的,包括离子表面活性剂,例如气溶胶邻联甲苯胺(Aerosol OT)、十二烷基苯磺酸钠、金属皂、聚丁烯琥珀酰亚胺、顺丁烯二酸酐共聚物、乙烯吡啶共聚物、乙烯吡咯烷酮共聚物(例如来自International Special Products的Ganex)、(甲基)丙烯酸共聚物、N,N-二甲基胺基乙基(甲基)丙烯酸乙酯(N,N-dimethylaminoethyl(meth)acrylate)共聚物。氟化表面活性剂在全氟化碳溶剂中作为电荷控制剂特别有用。这些包括了FC氟化表面活性剂,例如自3M公司的FC-170C、FC-171、FC-176、FC430、FC431和FC-740,以及Zonyl氟化表面活性剂,例如来自Dupont公司的Zonyl FSA、FSE、FSN、FSN-100、FSO、FSO-100、FSD和UR。
适当的带电颜料分散物可以通过任何已知的方法制造,包括研磨、碾磨、球磨、气流磨(microfluidizing)、以及超声波技术。例如,将细微粉末形式的颜料微粒添加到该悬浮溶剂中,所形成的混合物经球磨或研磨数小时,而将高度团聚的干颜料粉末粉碎成最初的微粒。虽然不是优选的方法,但是在球磨过程中,用于产生悬浮介质颜色的染料或颜料可以添加到该悬浮物中。
可通过使用适当的聚合物将该微粒微囊化,以消除颜料微粒的沉淀或乳化,使其比重与介电溶剂的比重一致。可用化学或物理方法完成颜料微粒的微囊化。典型的微囊化工艺包括界面聚合、原位聚合、相分离、凝聚、静电涂布、喷雾干燥、流化床涂布、以及溶剂蒸发。
就黑/白的电泳显示器而言,该悬浮物包含分散于黑色溶剂中的带电荷的白色二氧化钛(TiO2)微粒,或分散于一种介电溶剂中的带电荷黑色微粒。黑色染料或染料混合物可被用于产生溶剂的黑色,如Pylam Products公司(亚利桑那州)的Pylam Spirit黑和FastSpirit黑,Aldrich公司的苏丹黑B,BASF公司的Thermoplastic BlackX-70,或一种不可溶的黑色颜料如碳黑。对于其它有色悬浮物来说,有多种可能性。对于减色系统而言,带电荷的二氧化钛(TiO2)微粒可悬浮于蓝绿色、黄色、或品红色的介电溶剂中。该蓝绿色、黄色、或品红色可使用染料或颜料产生。对于加色系统而言,带电荷的二氧化钛微粒可悬浮于红色、绿色、或蓝色的介电溶剂中,其中该红色、绿色、或蓝色亦可使用染料或颜料产生。大多数的应用最好采用这种红色、绿色、或蓝色系统。
III.微型杯的密封
微型杯的密封可以通过多种方法完成。一种优选的方法是将包含有多官能团的丙烯酸酯、丙烯酸低聚物、和光引发剂的紫外光可固化组分分散在包含有带电荷颜料微粒和经染色的介电溶剂的电泳流体中。该紫外光可固化组分与该介电溶剂是不互溶的,且其比重低于该介电溶剂和颜料微粒。这两个组分(紫外光可固化组分和电泳流体)在一个径向混合器中充分地混合,并采用Myrad棒、凹印板、刮刀片、开槽涂布、或开缝涂布等精确的涂布机械装置,立即涂布到该微型杯上。多余的流体用刮刀或类似的装置刮除。少量的弱溶剂或者溶剂混合物例,如异丙醇、甲醇、或其他水性溶液溶剂可以用于清洗该微型杯的分隔壁顶表面上残留的电泳流体。挥发性的有机溶剂可以用于控制该电泳流体的粘性和覆盖性。然后将经过填充的微型杯烘干,且该紫外光可固化组分漂浮到该电泳流体的顶端。通过在该浮至表面的紫外光可固化层浮到顶端的期间或之后,将其固化,密封该微型杯。紫外光或可见光、红外线、及电子束等其它形式的辐射都可以用于将该微型杯固化并密封。此外,热或湿气也可以用于将该微型杯固化并密封,如果合适的话,可使用热或湿气固化组分。
优选介电溶剂组(具有理想的密度,且对丙烯酸酯单体和低聚物有理想的溶解度差别)是卤化碳氢化物及其衍生物。表面活性剂可用以改良该电泳流体和密封材料之间界面的粘性和润湿性。有用的表面活性剂包括3M公司的FC表面活性剂、DuPont公司的Zonyl氟化表面活性剂、氟化丙烯酸酯、氟化甲基丙烯酸酯、氟取代长链醇类、全氟取代的长链羧酸及其衍生物。
此外,如果这种密封前体物至少部分地与介电溶剂相容,则可将电泳流体及密封前体物依次涂布于微型杯。这样,可通过涂敷一层热固性前体物薄层(该前体物是辐射、热、湿气、或界面反应可固化的),并将其固化于经填充的微型杯表面,以完成密封过程。界面聚合后进行紫外光固化,对于密封过程极为有利。通过界面聚合形成一个薄的分隔层,使电泳层与外敷层之间的互相混合明显地得到抑制。接着通过后固化步骤完成密封,优选为紫外光辐射或其他光辐射。为进一步降低互混程度,最好外涂敷层的比重明显低于电泳流体的比重。可用挥发性有机溶剂调整涂层的粘度和厚度。当挥发性溶剂用于外涂敷层时,优选与该介电溶剂不相混溶的挥发性溶剂。这种二步涂敷方法,对所用染料至少部分地溶解于热固性前体物情形特别适用。
IV.单色电泳显示器的制备
通过图6所示的流程图说明此工艺。所有的微型杯都用同色组分的悬浮物填充。该工艺可以是连续的辊对辊工艺,包括下列步骤:
1.在一导电膜(61)上涂布一层非必选带有溶剂的热塑性或热固性前体物(60)。如果有溶剂,则该溶剂很容易挥发。
2.在高于该热塑性或热固性前体物层的玻璃化温度下,将该热塑性或热固性前体物层通过一预成形的凸模(62)进行模压。
3.将模具从热塑性或热固性前体物层脱模,优选在硬化的期间或之后。
4.将这样制成的微型杯(63)阵列用经染色的介电溶剂(64)填充,其中该介电溶剂包含有至少一种与该溶剂不相溶并具有比该溶剂和颜料微粒比重小的热固性前体物。
5.在该热固性前体物分离并在液相顶端形成一悬浮层的期间或之后,优选紫外光辐射(65),或者用热或湿气,将热固性前体物固化而密封该微型杯,这样形成装有分散在一经染色介电溶剂中的颜料悬浮物的密封电泳盒。
6.将预涂布有一胶层(67)的第二导电膜(66)层叠在经密封的电泳盒阵列上,其中该胶层(67)可以是压敏粘合剂、热熔粘合剂,热、湿气、或辐射固化粘合剂。
该如果该顶端导电层是透明的,则该层叠的粘合剂可以通过紫外光(68)等辐射透过该顶端导电膜而进行后固化。在该层叠步骤完成后,就可以切割为成品(69)。
上述的微型杯制备可以很容易地用另一种方法取代:对涂布有热固性前体物的导电膜进行图形曝光,然后用适当的溶剂将该未曝光区域去除。也可以通过在电泳流体表面直接涂布并固化一层热固性前体物组分来完成对微型杯的密封。
V.多色电泳显示器的制备
对于制造多色电泳显示器而言,需要附加的步骤以产生包含不同颜色悬浮物的微型杯。这些附加的步骤包括:(1)将一正性作用干膜光致抗蚀剂层叠在已制成的微型杯上,其中该光致抗蚀剂至少包含有一种可去除载体,例如Saint-Gobain公司(Worcester,MA)PET-4851,Shipley公司的酚醛正性光致抗蚀剂Microposit S1818,以及National Starch公司的Nacor72-8685和BF Goodrich公司的Carboset 515的混合物—一种碱性显影胶层;(2)通过将该光致抗蚀剂进行图形曝光,将可去除的载体膜去除,以及用例如Shipley公司的经稀释的Microposit 351显影剂将该正性光致抗蚀剂显影,选择性地开启一定数目的该微型杯;(3)用含有带电荷白色颜料(二氧化钛)微粒的电泳流体和该第一原色的染料或颜料填充该已经开启的微型杯;并且(4)按照制作单色显示器中的方法,将该经填充的微型杯密封。这些额外的步骤可以重复,以便制作第二和第三原色电泳流体填充的微型杯。
更特别地,多色电泳显示器可根据图7所示的步骤来制作。
1.在一导电膜(71)上涂布一层热固性前体物(70)。
2.在高于热塑性或热固性前体物层的玻璃化温度下,将该热塑性或热固性前体物层通过一预成形的凸模(图中未示出)进行模压。
3.将模具从热塑性或热固性前体物层脱模,优选是在通过冷却硬化,或通过辐射、热、或湿气进行交联硬化的期间或之后。
4.层叠一正性干膜光致抗蚀剂于所制成的微型杯(72)阵列上,其中该光致抗蚀剂层包含至少一胶层(73)、一正性光致抗蚀剂层(74)以及一可去的除塑料保护片(图中未示出)。
5.将该正性光致抗蚀剂用紫外光、可见光或其他辐射进行图形曝光(图7c),去除塑料保护片,在曝光区域显影并打开微型杯。步骤4及步骤5的目的是在一预定区域有选择地打开微型杯(图7d)。
6.用分散在介电溶剂中的带电荷白色颜料分散物(75)填充该打开的微型杯,其中该介电溶剂至少包含该第一原色的染料或颜料,以及与该溶剂不相溶并具有比该溶剂和颜料微粒比重低的热固性前体物(76)。
7.在该热固性前体物分离并形成一漂浮在该液相顶端的表面层期间或之后,通过将该热固性前体物固化(最好通过紫外光辐射,通过热或湿气的方法次之)把该微型杯密封,从而形成含有该第一原色的电泳流体的密封电泳盒(图7e)。
8.可以重复上述的步骤5至7,从而在不同区域产生包含有不同颜色电泳流体的明确定义的盒(图7e,7f与7g)。
9.将预涂布有一胶层(78)的一个预制图形的第二预透明导电膜(77)套准、层叠于密封的电泳盒阵列上,其中胶层(78)可以是压敏粘合剂,热熔粘合剂,热、湿气、或辐射固化粘合剂。
10.将该粘合剂固化。
以上方法中该微型杯的制作可以容易地用另一种方法取代:将涂布有一热固性前体物的导电膜进行图形曝光,然后用适当的溶剂将该未曝光区域去除。该微型杯的密封还可以通过在液相表面直接地涂布并固化热固性前体物材料来完成。
用本方法制造的显示器可以达到仅一张纸的厚度。该显示器的宽度可为涂布片的宽度(通常为3至90英寸)。该显示器的长度可为数英寸至数千英尺,取决于卷的大小。
实施例
以下所描述的实施例,是为便于本领域技术人员能够更清楚地了解并实施本发明,不应理解为是对本发明范围的限制,而仅仅是对本发明的说明和示范。
实施例1 利用微模压法的微型杯制备
表1中所示的组分是用一个3密耳(千分之一英寸)开口的镍铬鸟型(Nickel Chrome bird type)薄膜涂布器,将其涂布在MylarJ101/200上。使溶剂挥发,留下一层玻璃化温度低于室温的粘性薄膜。
表1:用于微模压的含有聚甲基丙烯酸甲酯(PMMA)的组分
  编号   说明   成分   供货商   重量百分比
1 环氧丙烯酸酯 Ebecryl 3605   UCBChemicals 7.35
  2   单体   Sartomer SR205   Sartomer   9.59
3 氨基甲酸乙酯丙烯酸酯 Ebecryl 6700   UCBChemicals 4.87
  4   聚甲基丙烯酸甲酯   Elvacite 2051   ICI   9.11
  5   光引发剂   Darocur 1173   Ciba   1.45
  6   阳离子光引发剂   Cyracure UVI6976   Union Carbide   0.60
  7   溶剂   丙酮   Aldrich   67.03
  总数   100.00
用Colorado Spring,Photo Stencil公司的预成形模板作为该微模压用的凸模,用Henkel公司的Frekote 700-NC作为脱膜剂。然后,室温下用加压滚轮的模板对该经涂布的薄膜进行模压。接着用装有金属氟化物灯管(具有80毫瓦/平方厘米的强度,波长为365纳米)的Loctite Zeta 7410曝光装置,透过Mylar膜将涂布物进行紫外光固化约20分钟。然后将经模压的薄膜从模具中脱模,呈现明确定义的微型杯,通过光学轮廓测量和显微镜测量,该微型杯具有从60微米至120微米(200-400dpi(点/英寸))范围的横向尺寸,以及5微米至30微米范围的深度(图4a至图4c)。
实施例2
含有固态低聚物、单体和添加剂的组分如表2所示。该混合物的玻璃化温度也低于室温。如前例,该粘性涂层沉积在MylarJ101/200的顶端。模压可使用加热加压辊或层合机(laminator),在32℃和60℃进行。制得具有5至30微米深的明确定义的高分辨率微型杯(100至400dpi)。
表2:含有低聚物、单体、添加剂和溶剂的模压组分
  编号   说明   成分   供货商   重量百分比
  1   环氧丙烯酸酯   Ebecryl 3903   UCB Chemicals   17.21
  2   单体   HDODA   UCB Chemicals   8.61
  3   氨基甲酸乙酯丙烯酸酯   Ebecryl 4827   UCB Chemicals   2.87
  4   光引发剂   Irgacure 500   Ciba   1.43
  5   增滑剂   Ebecryl 1360   UCB Chemicals   1.60
  6   溶剂   丙酮   Aldrich   68.26
  总数   100.00
实施例3  介电溶剂中的颜料分散物的制备
聚苯乙烯(0.89克,Polysciences公司,分子量50,000)以及AOT(0.094克,American Cyanamide公司,琥珀酸二辛酯磺酸钠)溶解在17.77克的热二甲苯(Aldrich公司)中。添加Ti-Pure R-706(6.25克)到该溶液中,并在一研磨机中以200转/分钟(rpm)的速度研磨12小时以上。得到了低粘性、稳定的分散物。将油溶蓝N(0.25克,Aldrich)添加到该分散物中进行染色。然后将该悬浮物用一标准的电泳盒(包含有被一个24微米的间隔物所隔离的二块ITO导电板)测试。在80伏特下,可观察到高对比度的白色蓝色交替影像,该影像具有大约60赫兹的切换速率和8.5毫秒的浮现时间。
实施例4
重复实施例3的实验,不同之处是使用油溶红EGN(Oil RedEGN,Aldrich公司)和具有24微米间隔物的电泳盒。在60伏特下,可观察到高对比度的红色与白色交替影像,该影像具有大约60赫兹的切换速率和12毫秒的浮现时间。
实施例5
在溶液中用研磨机研磨Ti-Pure R-706(112克),其中该溶液包含有11.2克的顺丁烯二酸酐共聚物(Baker Hughes的X-5231)、24克的3,4-二氯三氟甲苯(3,4-dichlorobenzotrifluoride,自Aldrich)、以及24克的1,6-二氯己烷(也来自Aldrich)。相似地,12克的碳黑在100℃的溶液中研磨,该溶液含有1.2克的烷基化聚乙烯吡咯烷酮(alkylated polyvinylpyrrolidone)(自ISP的Ganex V216)、34克的3,4-二氯三氟甲苯、以及34克的1,6-二氯己烷(Aldrich)。然后,将这二种分散物均匀地混合并测试。在100伏特下,可观察到高对比度的黑色与白色交替影像,该影像具有最高10Hz的切换速率和约36毫秒的浮现时间。
实施例6  用一步法工艺密封微型杯
0.05毫升的含有占重量比1%的苯偶酰二甲基缩酮(benzildimethyl ketal,Sartomer公司的Esacure KB1)的1,6-己二醇二丙烯酸酯(HDDA,1,6-hexanediol diacrylate,来自Aldrich)紫外光可固化组分,分散在0.4毫升的介电溶液中,该介电溶液含有分散在FC-43(来自3M公司)中的占重量比0.5%的2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-氟代十九烷-1-癸醇(-nonadecafluoro-1-decanol)(Aldrich)。所产生的分散物立即填充在按实施例2制作的微型杯阵列中。多余的流体用刮刀刮除。该HDDA溶液发生相分离需要至少30秒,并用紫外光辐射(10毫瓦/平方厘米)进行固化约1分钟。在微型杯顶部可以观察到一坚硬清晰的薄层,并且该微型杯被密封。
实施例7  用二步法(涂布和紫外光固化)工艺密封微型杯
将实施例5中制备的电泳流体涂布在按实施例2方法制作的微型杯阵列上。将一个Norland光学粘合剂NOA 60(新泽西州NewBrunswick的Norland Products公司)薄层涂布在该经填充的微型杯上。任何多余的紫外光粘合剂要用Mylar膜薄刮片刮除,并用一片吸收纸清理。该经涂布的粘合剂立即在Loctite Zeta紫外光曝光装置下进行15分钟固化。该微型杯被完全密封,且看不到气泡。用Mitutoyo公司的厚度计测量的,该经固化的胶层厚度约为5至10微米。
实施例8  用二步法(涂布和湿气固化)工艺密封微型杯
重复实施例7的实验,不同之处是用俄亥俄州哥伦布Elmer’sProducts公司的Instant Krazy胶替代该Norland粘合剂。涂布的粘合剂用空气中的湿气固化5分钟。该微型杯被完全地密封,看不到气泡。用Mitutoyo公司的厚度计测量,该经固化的胶层厚度约为5至10微米。
实施例9  用二步法(涂布和界面聚合)工艺密封微型杯
重复实施例8的实验,不同之处是用含有占重量0.3%的四乙撑五胺(Aldrich)的3,4-二氯三氟甲苯(3,4-dichlorobenzotrifluoride)溶液代替该电泳流体,用无水醚中的脂肪族聚异氰酸酯(来自Bayer公司的聚氨基甲酸酯类粘合剂N 3300)溶液代替该Instant Krazy胶。在涂布之后几乎可以立即观察到一个高度交联的薄膜。醚在室温下蒸发后,该介电溶液被完全地密封在微型杯中。没有观察到气泡。
虽然本发明已通过参考其特定具体实施例来说明,但是对于本领域技术人员来说,可以容易地对上述实施方案进行各种改变和等同置换而不偏离本发明的目的、精神、和范围。另外,可以有许多修改以适用于特别的情形、材料、组分、方法、方法步骤或步骤,而不脱离本发明的目的、精神、与范围。所有这类修改被认为在所附权利要求的范围内。
组件符号说明
10 电极板
11 电极板
12 盒层
20 凸模
2  透明导电膜
22 热塑性或热固性前体物层
23 微型杯阵列
24 腹板
30 玻璃基板
31 籽金属薄层
32 光致抗蚀剂层
33 镍钴合金
34 光掩模
50 光掩模
51 辐射固化材料
52 导电膜
53 塑料基板
54 深色的方块
55 无遮挡的区域
56 微型杯
60 热固性前体物层
61 导电膜
62 凸模
63 微型杯
64 介电溶剂
65 紫外光辐射
66 第二导电膜
67 胶层
68 紫外光(UV)辐射
69 切割
70 热固性前体物
71 导电膜
72 微型杯
73 胶层
74 正性光致抗蚀剂
75 颜料分散物
76 热固性前体物
77 透明导电膜
78 胶层

Claims (10)

1.一种用于制造多色电泳显示器的方法,包括以下步骤:
a)制备微型杯;
b)将所述微型杯层叠一层正性光致抗蚀剂;
c)将所述的正性光致抗蚀剂进行图形曝光,在预定区域中有选择地打开微型杯;
d)将打开的微型杯用电泳流体填充,所述电泳流体包含分散于第一色的介电溶剂中的带电荷颜料微粒;
e)将经填充的所述微型杯密封;
f)在不同的区域中重复步骤c)至e),从而产生填充有不同颜色的电泳流体的微型杯组;以及
g)如果有,则去除残留的正性光致抗蚀剂。
2.根据权利要求1所述的方法,其中所述的微型杯的填充和密封是通过以下方式完成的:用含有热塑性或热固性前体物的电泳流体填充所述的微型杯,其中所述热塑性或热固性前体物的比重低于所述介电溶剂和带电荷颜料微粒的比重,硬化在所述电泳流体的顶部由所述热塑性或热固性前体物形成的漂浮层。
3.根据权利要求2所述的方法,其中其中所述的硬化是通过溶剂蒸发、界面反应、湿气、热、辐射、或者其结合的方法完成的。
4.根据权利要求2所述的方法,其中所述的热塑性或热固性前体物与所述的介电溶剂不互溶。
5.根据权利要求1所述的方法,其中所述的密封是通过在所述的电泳流体上涂布包含热塑性或热固性前体物的组分,所述热塑性或热固性前体物的比重低于所述介电溶剂和带电荷颜料微粒的比重,并硬化所述热塑性或热固性前体物的组分完成的。
6.根据权利要求5所述的方法,其中所述的硬化是通过溶剂蒸发、界面反应、湿气、热、辐射、或者其结合的方法完成的。
7.根据权利要求5所述的方法,其中所述的热塑性或热固性前体物与所述的介电溶剂不互溶。
8.根据权利要求1所述的方法,其中所述的微型杯是通过用凸模将一热塑性或热固性前体物层进行模压或者将一辐射固化材料层进行图形曝光再去除未曝光区域制备的。
9.根据权利要求1所述的方法,其中一胶层被预先涂敷在所述正性光致抗蚀剂上并被层叠在所述微型杯上。
10.根据权利要求9所述的电泳显示器,其中所述的胶层可被所述正性光致抗蚀剂的显影剂显影。
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JP3680996B2 (ja) 2005-08-10
KR100566417B1 (ko) 2006-04-04
EP1264210B1 (en) 2004-11-24
CN1363056A (zh) 2002-08-07
EP1264210A1 (en) 2002-12-11
US20020131152A1 (en) 2002-09-19

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